Isolation, structure elucidation, and high‐performance liquid chromatography quantification of photolytic degradation impurities in acrivastine

Acrivastine is a second‐generation H1‐receptor antagonist, and its structure is sensitive to ultraviolet. Four unknown and one reported degradation products can be detected in the ultraviolet radiation solutions of acrivastine. To improve the quality control of acrivastine, the photodegradation impu...

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Bibliographic Details
Published in:Journal of separation science 2022-09, Vol.45 (18), p.3480-3490
Main Authors: Lv, Jun‐Jiang, Yu, Jia, Zeng, Xiao‐Yan, Zeng, Xue, Li, Yan, He, Dong‐Xian, Lin, Yi‐Min
Format: Article
Language:English
Subjects:
acrivastine
Chromatography
Impurities
Ions
Liquid chromatography
NMR spectroscopy
Photodegradation
photolytic degradation
Quality control
Silica gel
Spectrum analysis
structure elucidation
Ultraviolet radiation
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Summary:Acrivastine is a second‐generation H1‐receptor antagonist, and its structure is sensitive to ultraviolet. Four unknown and one reported degradation products can be detected in the ultraviolet radiation solutions of acrivastine. To improve the quality control of acrivastine, the photodegradation impurities were isolated and structurally elucidated. There are four new impurities (1–3 and 5), and one reported compound (4). The isolation strategy was designed as preparative high‐performance liquid chromatography using a reversed phase column with volatile acid addition in the mobile phase, combined with preparative thin‐layer chromatography using silica gel with alkaline addition in the mobile phase. Using the developed methods, five impurities (1–5) were efficiently purified after two or three chromatography runs with purities > 95%. The structures of compounds 1–5 are elucidated based on spectroscopy analysis of MS, and nuclear magnetic resonance spectroscopy. Using the impurity standard, the high‐performance liquid chromatography method was developed and validated. The method was proved to be sensitive, accurate (Recovery% 96.1–107.7%), linear (0.15–0.75 μg/mL, R2 > 0.996), robust, and specific, and it was successfully used to determine the degradation impurities of acrivastine and its formulation.
ISSN:1615-9306
1615-9314
DOI:10.1002/jssc.202200315